EP0417948A2 - Verfahren und Vorrichtung zur Ziehung eines Siliziumeinkristalles - Google Patents

Verfahren und Vorrichtung zur Ziehung eines Siliziumeinkristalles Download PDF

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Publication number
EP0417948A2
EP0417948A2 EP90309588A EP90309588A EP0417948A2 EP 0417948 A2 EP0417948 A2 EP 0417948A2 EP 90309588 A EP90309588 A EP 90309588A EP 90309588 A EP90309588 A EP 90309588A EP 0417948 A2 EP0417948 A2 EP 0417948A2
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EP
European Patent Office
Prior art keywords
silicon
single crystal
tube
melt
opaque
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Application number
EP90309588A
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English (en)
French (fr)
Other versions
EP0417948A3 (en
Inventor
Seizou C/O Nsc Electron Corporation Meguro
Hirofumi C/O Nsc Electron Corporation Harada
Ryuichi C/O Nippon Steel Corporation Habu
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Steel Corp
Siltronic Japan Corp
Original Assignee
Nippon Steel Corp
NSC Electron Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Nippon Steel Corp, NSC Electron Corp filed Critical Nippon Steel Corp
Publication of EP0417948A2 publication Critical patent/EP0417948A2/de
Publication of EP0417948A3 publication Critical patent/EP0417948A3/en
Withdrawn legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method

Definitions

  • This invention relates to a method and apparatus for pulling up a single crystal of silicon. More particularly, this invention relates, in the production of a single crystal of silicon by the Czochralski method, to a method and an apparatus for preventing the single crystal of silicon from being defiled with a metallic impurity and, at the same time, precluding the occurrence of oxidation-­induced stacking fault (OSF) in the single crystal of silicon.
  • OSF oxidation-­induced stacking fault
  • the CZ method which comprises growing and, at the same time, pulling up a crystal from a melt in a crucible is widely practiced.
  • the growth of a single crystal of silicon by this CZ method is started by charging a quartz crucible disposed in a chamber with prescribed amounts of raw materials such as polycrystalline silicon and a dopant and the like which are optionally added and heating the crucible with a heater encircling the crucible thereby melting the raw materials and forming a melt.
  • the growth is then accomplished by dipping in the melt of raw materials formed in the crucible a seed crystal attached to the leading end of a pulling wire and pulling up the wire while keeping the quarts crucible and the seed crystal rotated thereby growing a single crystal of silicon at the lower end of the seed crystal.
  • silicon monoxide SiO
  • SiO silicon monoxide
  • Japanese Patent Publication SHO 57(1982)-40, 119 has disclosed a method which, in the operation of the CZ method, comprises providing a single crystal of silicon in the process of being pulled up with a cover in the shape of an inverse cone having an axis coinciding with the axis of the single crystal of silicon and having a lower end thereof closely approximating the outer peripheral surface of the single crystal of silicon and the liquid surface of the melt thereby intercepting the heat of radiation from the crucible wall and allowing an addition to the pulling speed of the crystal and, at the same time, preventing the vapor of the melt from advancing to the upper part of the single crystal of silicon and precluding the possibility of the vapor condensing and falling onto the single crystal of silicon and compelling the single crystal to attain growth in a dislocated state.
  • the cover of the shape of an inverted cone, for the purpose of reflecting the heat of radiation, is made of such a metal as tungsten, niobium, tantalum, steel, nickel, or germanium.
  • An object of this invention is to provide an improved method and an apparatus for pulling up a single crystal of silicon.
  • Another object of this invention is to provide, in the production of a single crystal of silicon by the Czochralski method, a method and an apparatus for pulling up a single crystal of silicon, which prevent the single crystal of silicon from being defiled with impurities and, at the same time, precludes the occurrence of oxidation-induced stacking fault (OSF) in the single crystal of silicon.
  • OSF oxidation-induced stacking fault
  • this invention provides a method for pulling up a single crystal of silicon from a melt in a crucible, which method is characterized by. interposing between the single crystal of silicon in the process of being pulled up and the crucible a tube of the shape of an inverted cone having the lower end thereof disposed in close approximation to the outer peripheral surface of the single crystal of silicon and the liquid surface of the melt and having at least the surface thereof formed of a nonmetallic substance, the lower end part thereof formed of an opaque material, and the other parts thereof formed of a transparent material.
  • an apparatus for pulling up a single crystal of silicon from a melt in a crucible which apparatus is characterized by the fact that a tube of the shape of an inverted cone having at least the surface thereof formed of a nonmetallic substance, the lower end part thereof formed of an opaque material, and the other parts thereof formed of a transparent material is so disposed as to have the axis thereof coinciding with the pulling direction of the single crystal of silicon and the lower end thereof falling in close approximation to the outer peripheral surface of the single crystal of silicon and the liquid surface of the melt.
  • the present invention in the production of a single crystal of silicon in accordance with the Czochralski (CZ) method, improves the pulling speed of the single crystal, prevents the occurrence of crystal fault and improves the freeing ratio of the single crystal during the course of pulling, prevents the single crystal from metallic contamination and, at the same time, precludes the occurrence of oxidation-induced stacking fault in the single crystal owing to the provision in the upper part of the crucible containing the melt a tube of the shape of an inverted cone having at least the surface thereof formed of a nom-metallic material, the lower end part thereof formed of an opaque material, and the other parts thereof formed of a transparent material.
  • CZ Czochralski
  • a single crystal of silicon 3 is pulled up from a melt 2 formed in a crucible 1.
  • a tube 4 made of transparent quartz in the shape of an inverted cone is interposed as disposed around the single crystal 3 of silicon as the axis thereof.
  • An opaque ring 5 having the surface thereof formed of a nonmetallic material is attached to the inner peripheral surface of the lower end part of the inverted cone-shaped tube 4. This opaque ring 5 is so disposed that the lower end thereof falls in close approximation to the single crystal 3 of silicon and the melt 2.
  • the melt 2 is heated with a cylindrical heater 6 and is covered with an inner shield 7 and an outer shield 8 which are both cylindrical in shape.
  • the inverted cone-shaped tube is is supported on a supporting base 9 disposed on the inner shield 7 and the outer shield 8.
  • the reference numeral 10 stands for a seed crystal used for the growth of the single crystal.
  • the transparent part of the inverted cone-shaped tube 4 is desired to be formed of transparent quartz.
  • a material for the opaque part graphite or a ceramic substance may be used.
  • the transparent part and the opaque part of the inverted cone-shaped tube 4 are only required to have their surfaces formed of a nonmetallic material as mentioned above.
  • the opaque part may be formed of a metallic material if the metallic material was coated with quartz or a ceramic substance.
  • transparent refers to a substance pervious to the heat of radiation from the heater, the crucible, or the melt and the term "opaque" to a substance impervious to the heat of radiation.
  • the apparatus for pulling up a single crystal of silicon in the other embodiment illustrated in Fig. 2 is identical in construction with the embodiment illustrated in Fig. 1, excepting the inverted cone-shaped tube 4 has an opaque ring 5 of a nonmetallic material nipped between the lower end parts of an outer peripheral member 4a made of transparent quartz and an inner peripheral member 4b made of transparent quartz.
  • the fact that the opaque member of nonmetallic material attached to the lower end part of the inverted cone-shaped tube as in the present embodiment is advantageous in respect that it will contribute to preventing the melt from contamination.
  • the operation of pulling up the single crystal of silicon contemplated by the present invention is carried out by the use of the apparatus constructed as described above in accordance with the CZ method.
  • the cooling speed of various sites of the single crystal 3 of silicon is desired to be not more than 4°C/min in a temperature zone not exceeding 800°C.
  • the possibility of the vapor from the melt 2 causing dislocation in the single crystal 3 of silicon in the process of being pulled up can be precluded because the inverted cone-shaped tube 4 is interposed between the single crystal 3 of silicon and th crucible 1 as disposed in close approximation to the single crystal 3 of silicon and the melt 2 as illustrated in Figs. 1 and 2. Since the surface of the inverted cone-shaped tube 4 is made of a nonmetallic material, it gives rise to no reaction product on contact with the SiO vaporizing from the melt 2 and, therefore contributes to preventing the melt 2 from metallic contamination.
  • the single crystal 3 of silicon immediately after being pulled up the melt 2 is protected by the opaque part against the heat of radiation emanating from the melt 2 and the crucible 1 and, therefore, can be pulled up at a higher speed. Since the single crystal 3 of silicon further grown thereafter is properly protected by the transparent part, the cooling speed of the various sites of the single crystal 3 of silicon in the process of being pulled up can be adjusted to a proper level not exceeding 5°C/min and the occurrence of OSF can be precluded.
  • the length of the lower end part which is rendered opaque depends on the conditions for growth such as the pulling speed of the single crystal 3 of silicon, the temperature of the melt, and the diameter of the single crystal being pulled up or on the size of the inverted cone-­shaped tube 4, the angle of inclination of the wall surface, and so on, it is generally desired to be such that the opaque lower end part rises to a height in the range of up to 8 cm, preferably up to 5 cm, above the liquid surface of the melt 2.
  • the length of the opaque lower end part has no particular restriction except for the sole requirement that it should contribute to improving the pulling speed as described above and avoid obstructing the retentio of the cooling speed at a level below 5°C/min.
  • a quartz crucible 1a having an inside diameter of 16 inches and reinforced externally with a graphite crucible 1b. From the melt, a single crystal 3 of silicon 130 mm in diameter was pulled up. An opaque ring 5 made of graphite was attached to the inner surface side of the lower end part of an inverted cone-shaped tube 4 made of transparent quartz.
  • Argon gas was passed through the gap between the single crystal 3 of silicon and the lower end of the inverted cone-­shaped tube 4 at a flow volume in the range of 15 to 100 liters/min in the direction of the arrow so as to maintain in the interior of the apparatus an argon gas atmosphere having an inner pressure in the range of 5 to 30 millibars.
  • the OSF density in the produced single crystal was conspicuously small as compared with that in the product of the comparative method as shown in Table 1.
  • the experiment of the convetional method was carried out by following the procedure of this example, excepting an inverted cone-shaped tube 4 was formed wholly of an opaque heat insulator.
  • the OSF density of a given single crystal of silicon was determined by heating the sample in a moist oxygen gas at 1,000°C for 60 minutes and subjecting the treated sample to visual observation under a microscope.
  • a quartz crucible 1a having an inside diameter of 16 inches and reinforced externally with a graphite crucible 1b. From the melt, a single crystal 3 of silicon 130 mm in diameter was pulled up.
  • An inverted cone-shaped tube 4 of transparent quartz was composed of an outer peripheral member 4a and an inner peripheral member 4b and had an opaque ring 5 of graphite nipped between the lower end parts of the two members mentioned above.
  • Argon gas was passed through the gap between the single crystal 3 of silicon and the lower ends of the inverted cone-shaped tube 4 at a flow volume in the range of 15 to 100 liters/min in the direction of the arrow so as to maintain in the apparatus an argon gas atmosphere having an inner pressure in the range of 5 to 30 millibars

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
EP19900309588 1989-08-31 1990-08-31 Method and apparatus for pulling up silicon single crystal Withdrawn EP0417948A3 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP225913/89 1989-08-31
JP22591389A JPH0388794A (ja) 1989-08-31 1989-08-31 シリコン単結晶の引上げ方法および装置

Publications (2)

Publication Number Publication Date
EP0417948A2 true EP0417948A2 (de) 1991-03-20
EP0417948A3 EP0417948A3 (en) 1991-07-24

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Family Applications (1)

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EP19900309588 Withdrawn EP0417948A3 (en) 1989-08-31 1990-08-31 Method and apparatus for pulling up silicon single crystal

Country Status (2)

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EP (1) EP0417948A3 (de)
JP (1) JPH0388794A (de)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0538048A1 (de) * 1991-10-17 1993-04-21 Shin-Etsu Handotai Company Limited Vorrichtung zur Einkristallziehung
DE19539316A1 (de) * 1995-09-26 1997-03-27 Leybold Ag Kristallziehanlage
EP0768392A2 (de) * 1995-10-11 1997-04-16 International Superconductivity Technology Center Vorrichtung zur Herstellung von Kristallen
US5707447A (en) * 1995-09-26 1998-01-13 Balzers Und Leybold Deutschland Holding Ag Crystal pulling apparatus
US7067007B2 (en) * 2002-08-24 2006-06-27 Schott Glas Process and device for growing single crystals

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2686223B2 (ja) * 1993-11-30 1997-12-08 住友シチックス株式会社 単結晶製造装置
US5683505A (en) * 1994-11-08 1997-11-04 Sumitomo Sitix Corporation Process for producing single crystals
JP2007314375A (ja) * 2006-05-26 2007-12-06 Shin Etsu Handotai Co Ltd 単結晶製造装置
CN111519241B (zh) * 2019-02-01 2021-12-17 上海新昇半导体科技有限公司 一种半导体晶体生长装置

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2942057A1 (de) * 1978-10-17 1980-04-24 Vlsi Technology Res Ass Verfahren und vorrichtung zur herstellung eines einkristall-siliziumstabs
EP0229322A2 (de) * 1985-12-11 1987-07-22 Shin-Etsu Handotai Company Limited Verfahren und Vorrichtung zum Herstellen von Einkristallen nach dem Czochralski-Verfahren
EP0320115A1 (de) * 1987-12-08 1989-06-14 Nkk Corporation Verfahren und Vorrichtung zur Herstellung von Siliciumeinkristallen

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2942057A1 (de) * 1978-10-17 1980-04-24 Vlsi Technology Res Ass Verfahren und vorrichtung zur herstellung eines einkristall-siliziumstabs
EP0229322A2 (de) * 1985-12-11 1987-07-22 Shin-Etsu Handotai Company Limited Verfahren und Vorrichtung zum Herstellen von Einkristallen nach dem Czochralski-Verfahren
EP0320115A1 (de) * 1987-12-08 1989-06-14 Nkk Corporation Verfahren und Vorrichtung zur Herstellung von Siliciumeinkristallen

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
IBM TECHNICAL DISCLOSURE BULLETIN, vol. 28, no. 1, June 1985, pages 211-212, New York, US; "Apparatus for low to medium level oxygen czochralski silicon crystal growth" *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0538048A1 (de) * 1991-10-17 1993-04-21 Shin-Etsu Handotai Company Limited Vorrichtung zur Einkristallziehung
DE19539316A1 (de) * 1995-09-26 1997-03-27 Leybold Ag Kristallziehanlage
US5707447A (en) * 1995-09-26 1998-01-13 Balzers Und Leybold Deutschland Holding Ag Crystal pulling apparatus
EP0768392A2 (de) * 1995-10-11 1997-04-16 International Superconductivity Technology Center Vorrichtung zur Herstellung von Kristallen
EP0768392A3 (de) * 1995-10-11 1998-04-01 International Superconductivity Technology Center Vorrichtung zur Herstellung von Kristallen
US7067007B2 (en) * 2002-08-24 2006-06-27 Schott Glas Process and device for growing single crystals

Also Published As

Publication number Publication date
EP0417948A3 (en) 1991-07-24
JPH0388794A (ja) 1991-04-15

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